4-Aminopyridine → HCID 9953049, compound

Participants

Reaction Steps

A homogenious mixture of 1.8 g (5.0 mmol) of 7-(3,5-dimethoxy-phenyl)-5-ethyl-3-methylsulfanyl-5H-pyrido[2,3-e]-1,2,4-triazin-6-one and 3.3 g (35.2 mmol) of 4-aminopyridine was heated at 150° C. for 2 days in a sealed reaction vessel, during which time the sublimed 4-aminopyrdine was reintroduced to the reaction mixture. At the end of 2 days, the sublimed 4-aminopyridine was removed, and the remaining mixture was triturated under 1:9 methanol/chloroform at room temperature and filtered. The solid was suspended in 60 mL of hot chloroform while methanol was added to produce a near homogeneous solution that was filtered and set aside for 6 days. The crystals were collected, washed with chloroform, and dried under house vacuum to give 610 mg (30%) of the title compound as yellow platelets. Mp=316-318° C. (dec).

Provenance & Evidence